Polyimide precursor solution composition

a technology of polyimide and solution composition, which is applied in the direction of electrode manufacturing process, cell components, coatings, etc., can solve the problems of insufficient properties, failure to disclose mechanical properties, and difficulty in producing satisfactory quality polyimide-resin-formed products, etc., to achieve stable solution viscosity, stable solution viscosity, and the effect of equal or superior properties

Active Publication Date: 2011-08-11
UBE CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0018]An object of the invention is to provide a polyimide precursor solution composition whose solution viscosity can easily be adjusted, that has a stable solution viscosity, and that can suitably produce polyimide-resin-formed products, such as polyimide films, having properties equal to or superior to those of straight-chain polyimides through heating at relatively low temperatures and / or in a short time.

Problems solved by technology

Among these, methods (b) and (c) employing chemical imidization can achieve imidization at relatively low temperatures, but the solution is prone to gelate, thus posing difficulty in producing polyimide-resin-formed products with satisfactory quality.
These Patent Documents, however, fail to disclose mechanical properties thereof.
However, the properties, such as the mechanical properties, of the polyimide-formed products obtained according to this method are not necessarily sufficient, and there still is room for improvement to suitably produce polyimide-resin-formed products, such as polyimide films, having properties equal to or superior to those of straight-chain polyimides through heating at relatively low temperatures and / or in a short time.
However, because of the large number of cross-linking points in the varnish, the resultant cross-linked polyimide tends to become hard and / or brittle, causing problems during use due to deterioration in flexibility, extensibility, and toughness compared to common polyimides.
Particularly, with so-called wholly aromatic polyimides having glass transition temperatures of 250° C. or higher and exhibiting excellent heat resistance and mechanical properties due to their stiff structures, there is difficulty in the heating step to suitably control the cross-linking reaction while, at the same time, increasing the molecular weight of the straight-chain polyimide segment to impart high physical properties, thus posing difficulty in suitably producing polyimide-resin-formed products, such as polyimide films, having excellent properties through heating at relatively low temperatures and / or in a short time.
However, the segment originating from the polyfunctional carboxylic acid compound will occupy a large volume fraction within the polyimide, thus creating a significant impact on the polyimide properties, such as disturbing the polyimide's crystalline properties, and posing difficulty in making the properties intrinsic to polyimides become evident, especially in highly-heat-resistant polyimide-formed products having glass transition temperatures of 250° C. or higher.
Therefore, it is difficult to suitably produce polyimide-resin-formed products, such as polyimide films, having properties equal to or superior to those of straight-chain polyimides through heating at relatively low temperatures and / or in a short time, especially in cases of highly-heat-resistant polyimide-resin-formed products.
Further, the polyfunctional carboxylic acid compound is neither commercially available nor easy to synthesize, thus difficult to obtain and extremely costly.

Method used

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  • Polyimide precursor solution composition
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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0122]To 221 g of N-methyl-2-pyrrolidone (also abbreviated hereinafter as “NMP”) was dissolved 20.02 g (0.100 mol) of 4,4′-diaminodiphenyl ether (also abbreviated hereinafter as “ODA”). To this solution was added 28.54 g (0.097 mol) of 3,3′,4,4′-biphenyltetracarboxylic dianhydride (also abbreviated hereinafter as “s-BPDA”), and the mixture was stirred for 24 hours at 25° C. until the s-BPDA dissolved and the solution became viscous, to obtain a solution of polyamic acid (A). The concentration of the polyamic acid in the solution was 18% by mass and the solution viscosity was 41 poise. To this solution was added 0.68 g (0.002 mol; 0.02 times by mole the number of moles of ODA) of mellitic acid, to prepare a polyimide precursor solution composition. The viscosity of the prepared polyimide precursor solution composition was 41 poise, which hardly changed after storage for 3 days at room temperature.

[0123]The prepared polyimide precursor solution composition was casted onto a glass plat...

example 2

[0128]To 221 g of NMP was dissolved 20.02 g (0.100 mol) of ODA. To this solution was added 28.54 g (0.097 mol) of s-BPDA, and the mixture was stirred for 24 hours at 25° C. until the s-BPDA dissolved and the solution became viscous, to obtain a solution of polyamic acid (A). The concentration of the polyamic acid in the solution was 18% by mass and the solution viscosity was 58 poise. To this solution were added, and dissolved evenly, 0.17 g (0.0005 mol; 0.005 times by mole the number of moles of ODA) of mellitic acid (which is 0.08 times by mole with respect to 0.006 mol which is the number of end amino groups of the polyamic acid if theoretical reaction occurs between ODA and s-BPDA) and 0.82 g (0.00225 mol; 0.0225 times by mole the number of moles of ODA) of s-BPTA, to prepare a polyimide precursor solution composition. The solution viscosity of the prepared polyimide precursor solution composition was 58 poise, which hardly changed after storage for 3 days at room temperature.

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example 3

[0130]A polyimide precursor solution composition was prepared in the same way as in Example 2, except that the amounts of mellitic acid and s-BPTA were changed to 0.34 g (0.001 mol) and 0.54 g (0.0015 mol), respectively. The solution viscosity of the prepared polyimide precursor solution composition was 58 poise, which hardly changed after storage for 3 days at room temperature.

[0131]The prepared polyimide precursor solution composition was casted onto a glass plate serving as a base material and dried with hot air for 30 minutes at 120° C. The dried film was peeled off from the glass plate, fixed in a metal frame, and heated for 10 minutes at 250° C. and for another 10 minutes at 300° C., to produce a 39-μm-thick polyimide film. Another polyimide film was produced by instead heating the dried film for 10 minutes at 250° C. and then for another 10 minutes at 350° C. The properties of the resultant polyimide films are shown in Table 2.

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Abstract

A first polyimide precursor solution composition contains: (A) a polyamic acid; (B) a carboxylic acid compound having at least three pairs of carboxyl groups within its molecule or an esterified product thereof; and (D) a solvent. A second polyimide precursor solution composition contains the components (A), (B), and (D) of the first polyimide precursor solution composition and additionally containing (C) a carboxylic acid compound having two pairs of carboxyl groups within its molecule or an esterified product thereof. A third polyimide precursor solution composition contains the components of the second polyimide precursor solution composition, wherein the polyamic acid (A) is a polyamic acid having a specific structure.

Description

TECHNICAL FIELD [0001]The present invention relates to a polyimide precursor solution composition containing a polyamic acid as a main component. The polyimide precursor solution composition of the invention can easily be adjusted in terms of solution viscosity, has a stable solution viscosity, and can suitably produce polyimide-resin-formed products, such as polyimide films, having properties equal to or superior to those of straight-chain polyimides through heating at relatively low temperatures and / or in a short time.[0002]The present invention also relates to a polyimide precursor solution composition that can produce a polyimide resin having excellent toughness, and to the polyimide resin produced therefrom. The polyimide resin produced from the polyimide precursor solution composition of the invention can suitably be used as formed products, such as endless belts, insulating protective films and other films, and as a binder resin for electrodes of electrochemical elements.BACK...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C08L77/06H01M4/62H01M4/04B05D5/12B05D3/02
CPCC08G73/1042C08G73/1046C08G73/105C08G73/1067C08G73/1071C08L79/08C08K5/1539H01M4/133H01M4/134H01M4/621H01M4/622C08K5/092C09D179/08Y02E60/10
Inventor HIRANO, TETSUJIKIDOSAKI, TORU
Owner UBE CORP
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